CN105038586A - Superhydrophobic paint, and preparation method and application thereof - Google Patents

Superhydrophobic paint, and preparation method and application thereof Download PDF

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CN105038586A
CN105038586A CN201510505184.1A CN201510505184A CN105038586A CN 105038586 A CN105038586 A CN 105038586A CN 201510505184 A CN201510505184 A CN 201510505184A CN 105038586 A CN105038586 A CN 105038586A
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nano level
super
hydrophobic coating
micro
hydrophobic
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CN105038586B (en
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侯仪
沈衡
赵宁
徐坚
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Institute of Chemistry CAS
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Institute of Chemistry CAS
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Abstract

The invention discloses a superhydrophobic paint, and a preparation method and application thereof. The preparation method of the micro/nano superhydrophobic paint comprises the following steps: 1) dissolving fluorinated polysiloxane in a solvent a to obtain a solution a; 2) dropwisely adding a solvent b into the solution a obtained in the step 1) to perform phase separation, wherein the obtained system is the micro/nano superhydrophobic paint; and centrifuging the micro/nano superhydrophobic paint to obtain the nano superhydrophobic paint. After the two paints are applied onto various substrates by dip coating or spray coating, the substrates can be superhydrophobic; and the paint can be used for self-cleaning materials, waterproof materials, oil-water separation materials and the like. Besides, the superhydrophobic material prepared from the paint has the characteristics of solvent resistance, acid/alkali resistance, friction resistance, high temperature resistance (up to 400 DEG C) and the like.

Description

Super hydrophobic coating and preparation method thereof and application
Technical field
The invention belongs to paint field, relate to a kind of super hydrophobic coating and preparation method thereof and application.
Background technology
Super-hydrophobicly refer to that water droplet is greater than 150 ° at the static contact angle of body surface, the phenomenon that roll angle is less than 10 °.Constructing super-drainage surface will meet two conditions usually: micro-nano multi-level structure and low surface energy.In recent years, super hydrophobic surface was widely used in the fields such as automatically cleaning, waterproof and oily water separation.But, most of super hydrophobic material not only complicated process of preparation, and the microstructure of material surface is very easily destroyed, makes super-hydrophobicity in use be difficult to keep.
Summary of the invention
The object of this invention is to provide a kind of super hydrophobic coating and preparation method thereof and application.
The invention provides a kind of method preparing micro/nano level super hydrophobic coating, comprise the steps:
1) fluorinated silicones is dissolved in solvent a, obtain solution a;
2) to step 1) add solvent b in the mode dripped in gained solution a and be separated, gained system is described micro/nano level super hydrophobic coating;
Described solvent a is selected from least one in the minority ketones such as tetrahydrofuran (THF), acetone, ethyl acetate, butanone and esters solvent;
Described solvent b is selected from least one in the alcohols such as methyl alcohol, ethanol, Virahol, water, toluene, dimethylbenzene, normal hexane, hexanaphthene or varsol; Solvent b is the non-solvent of fluorinated silicones.
In aforesaid method, described fluorinated silicones is the polysiloxane that side chain contains fluorine atom, is specifically selected from least one in trifluompropyl methyl polysiloxane (PTFPMS), poly-methyl nine fluorine hexyl siloxanes (PNFHMS), poly-ten trifluoro caprylil methicone (PTDFOMS) and poly-methyl 17 fluorine decyl siloxanes (PHDFDMS);
Wherein, the weight-average molecular weight of described trifluompropyl methyl polysiloxane (PTFPMS) is 3000 – 1,000,000, specifically can be 5000-5 ten thousand, more specifically can be 10,000;
The weight-average molecular weight of described poly-methyl nine fluorine hexyl siloxanes (PNFHMS) is 4000-200 ten thousand, specifically can be 5000-5 ten thousand, more specifically can be 20,000;
The weight-average molecular weight of described poly-ten trifluoro caprylil methicone (PTDFOMS) is 5000-250 ten thousand;
The weight-average molecular weight of described poly-methyl 17 fluorine decyl siloxanes (PHDFDMS) is 6000-300 ten thousand;
In described solution a, the concentration of fluorinated silicones is 0.1-200mg/ml, preferably 25 – 50mg/ml;
The mass ratio of described fluorinated silicones and described solvent b is 1:10-10000, preferred 1:20-600.
Described step 1) in, the mode of dissolving is stirring and dissolving; The rotating speed stirred is 100-3000rpm, is specially 800-1000rpm; The time of stirring is 1-30 days, is specially 5 days;
Described step 2) drip in step, the speed of dropping is within 1 second 1, drop to 1 second 10;
The mode be separated is for stirring; The rotating speed stirred is 100-3000rpm, and being specially 500-1000rpm, is more specifically 500rpm, 700rpm, 900rpm, 1000rpm.
In addition, the micro/nano level super hydrophobic coating prepared according to the method described above, also belongs to protection scope of the present invention.Wherein, in described micro/nano level super hydrophobic coating, the particle diameter of aggregate is 20nm – 20 μm.This aggregate is specially fluorinated silicones aggregate.
Present invention also offers a kind of method preparing nano level super hydrophobic coating, comprise the steps: centrifugal for aforementioned micro/nano level super hydrophobic coating provided by the invention, collect centrifugal after the supernatant liquid that obtains, obtain described nano level super hydrophobic coating.
In the centrifugation step of aforesaid method, centrifugal rotational speed is 500rpm-12000rpm, centrifugation time 5min-30min, and centrifugal radius is 6-12cm.
In addition, the nano level super hydrophobic coating prepared according to the method described above, also belongs to protection scope of the present invention.
In described nano level super hydrophobic coating, the particle diameter of aggregate is 20nm-100nm.This aggregate is specially fluorinated silicones aggregate; This nano level super hydrophobic coating presents micro-blue opalescence.
Present invention also offers the application of above-mentioned super hydrophobic coating.
Be specially; the micro/nano level super hydrophobic coating that the invention described above provides or nano level super hydrophobic coating in the application prepared in superhydrophobic article and; the application of above-mentioned nano level super hydrophobic coating in the super-hydrophobic filter membrane of preparation or the superhydrophobic article prepared by described micro/nano level super hydrophobic coating or nano level super hydrophobic coating or the super-hydrophobic filter membrane prepared by nano level super hydrophobic coating, also belong to protection scope of the present invention.
Wherein, the aperture of described superhydrophobic article is 1 μm-1000 μm;
The aperture of described super-hydrophobic filter membrane is 20nm-900nm, specifically can be 220nm-450nm.
The method preparing superhydrophobic article provided by the invention, comprises the steps:
Aforementioned micro/nano level super hydrophobic coating provided by the invention is flooded or is sprayed in substrate, dry, obtain described superhydrophobic article.
In aforesaid method, the material forming described substrate is fiber or porous material, is specially fabric, sponge, metal screen or filter paper; Wherein, described fabric is natural fabric or synthetic textile, and described natural fabric is specially cotton, fiber crops, silk or hair textiles; Described synthetic textile is terylene, polypropylene fibre, polyamide fibre, spandex or acrylic fibers textiles; Described sponge is polyester, polyvinyl alcohol foam sponge or polyethers sponge; Described metal screen to be mean pore size the be stainless (steel) wire of 30 μm-1000 μm; Described filter paper is qualitative filter paper or quantitative paper;
In described drying step, temperature is 25-100 DEG C, and the time is 1h-24h, specifically can be 2h or 3h.
The method of the super-hydrophobic filter membrane of preparation provided by the invention, comprises the steps:
Aforementioned nano level super hydrophobic coating provided by the invention is coated on filter membrane under vacuum, dry, obtain described super-hydrophobic filter membrane.
In aforesaid method, the aperture of filter membrane is 20nm-900nm, specifically can be 220nm-450nm;
Described filter membrane is nylon membrane, poly tetrafluoroethylene, polyvinylidene fluoride film, blend fiber ester film, glass fibre membrane, di-aluminium trioxide film, polyamide membrane, cellulose acetate membrane, polysulfone membrane, poly (ether sulfone) film or polyvinyl alcohol film;
In described vacuum condition, vacuum tightness is 0.02-0.1MPa;
In described drying step, temperature is 30-100 DEG C, and the time is 1h-24h, specifically can be 2h or 3h.
In addition, the superhydrophobic article prepared according to the method described above or super-hydrophobic filter membrane and this superhydrophobic article or the application of super-hydrophobic filter membrane in oily water separation, also belong to the scope of protection of present invention.Wherein, described superhydrophobic article is the superhydrophobic article with at least one in following performance: solvent resistant, acid and alkali-resistance, high temperature resistant and mechanical resistant friction;
Wherein, described high temperature resistant be the temperature of the highest tolerance 400 DEG C.
Described oily water separation specifically can comprise the steps:
1) poured into by the oil-water mixture of certain volume ratio in the tripping device clamping super-hydrophobic substrate, under gravity, oil is by super-hydrophobic substrate, and water is trapped within substrate, realizes the separation of oil-water mixture.
2) pour in the tripping device being fixed with super-hydrophobic substrate by the high temperature oil water mixture of certain volume ratio, under gravity, oil is by super-hydrophobic substrate, and water is trapped within substrate, achieves the separation of high temperature oil water mixture.
3) pour water-in-oil emulsion into tripping device, this tripping device clamps super-hydrophobic filter membrane, and under certain vacuum pressure, the oil phase in emulsion, by filter membrane, obtains the filtrate of clarification, achieves the separation of water-in-oil emulsion.
Step 1) described oil is common with the immiscible organic solvent of water, oil fuel, edible wet goods.The volume ratio of described oil-water mixture is not limit.
Step 1) described in super-hydrophobic substrate be fiber or porous material, be specifically as follows fabric, sponge, metal screen, filter paper etc.
Step 2) described in high temperature oil water mixture temperature be 90 – 100 DEG C.
Step 3) described in water-in-oil emulsion comprise the water-in-oil emulsion of surfactants stabilize and the water-in-oil emulsion of surfactant-free.Oil is common with the immiscible organic solvent of water, oil fuel, edible wet goods.
Step 3) described in nanoporous filter membrane comprise the nylon membrane of aperture between 20nm-900nm, poly tetrafluoroethylene, polyvinylidene fluoride film, blend fiber ester film, glass fibre membrane, di-aluminium trioxide film, polyamide membrane, cellulose acetate membrane, polysulfone membrane, poly (ether sulfone) film, polyvinyl alcohol film etc.
Described solvent resistant specifically refers to the aforementioned superhydrophobic article obtained by micro/nano level super hydrophobic coating provided by the invention at room temperature warp 60co is that the gammairradiation 10min of the 100kGy of light source carries out cross-linking radiation, it is greater than 150 ° to the contact angle of water to superhydrophobic article after crosslinked after tested, after the ketone such as tetrahydrofuran (THF), acetoneand ethyl acetate or esters solvent soak, still keep super-hydrophobicity.
Described acid and alkali-resistance specifically refers to the surface acid of certain pH value, alkali, salt brine solution being dripped to respectively the aforementioned superhydrophobic article obtained by micro/nano level super hydrophobic coating provided by the invention, the drop of acid, alkali, salt can easily from its surperficial landing, this superhydrophobic article is all greater than 150 ° to the contact angle of acid, alkali, salt after tested, has the characteristic of acid and alkali-resistance.Wherein, the pH value range of described acid, alkali, salt brine solution is 1 – 14, is specially the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7.
The aforementioned inorganic or metal super-hydrophobic goods obtained by micro/nano level super hydrophobic coating provided by the invention are placed in retort furnace (lower than 400 DEG C) calcining 1-5h by described high temperature resistant specifically referring to, the contact angle of goods after calcining to water is greater than 150 °, has resistant to elevated temperatures characteristic.
Described mechanical resistant friction specifically refers to the weight by the aforementioned superhydrophobic article obtained by micro/nano level super hydrophobic coating provided by the invention being placed certainweight, in certain distance, make it after coated abrasive surface circulation friction for several times, after tested, the contact angle of goods after friction to water is greater than 150 °, has the characteristic of mechanical resistant friction.Wherein, the weight of described load can be 100 – 250g, and described rub cycle number of times is 10 – 100 times, and described frictional distance is 10 – 30cm.
Outstanding advantages of the present invention is:
1, the preparation method of micro/nano level super hydrophobic coating and nano level super hydrophobic coating is simple, only needs to add non-solvent at normal temperatures and just can obtain.
2, the preparation method of superhydrophobic article is easy, only need dip-coating in substrate, spray this dispersion liquid A or under certain vacuum pressure, nano level super hydrophobic coating be coated on porous membrane, then make solvent evaporates at normal temperatures, substrate just can be made to possess super-hydrophobic character.
3, the method has universality, and two kinds of super hydrophobic coatings all can be coated in the substrate of any material, give the characteristic that it is super-hydrophobic.
4, the characteristic such as acid and alkali-resistance, solvent resistant, mechanical resistant friction, high temperature resistant (reaching as high as 400 DEG C) is possessed by the super hydrophobic material of these two kinds of super hydrophobic coating modifications.
5, the substrate of these two kinds of super hydrophobic coating modifications is utilized to be used as self-cleaning material, water-proof material, oily water separation material etc.; In addition, the superhydrophobic article obtained by this coating also has the characteristic such as solvent resistant, acid and alkali-resistance, mechanical resistant friction, high temperature resistant (reaching as high as 400 DEG C).
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the super-hydrophobic gauze of preparation in embodiment 1, and magnification is 330 times.
Fig. 2 is the result figure of super-hydrophobic gauze oil-water separation mixture in embodiment 1.
Fig. 3 is photo and the optical microscope picture that water-in-oil emulsion is separated front and back.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described starting material all can obtain from open commercial sources if no special instructions.
Embodiment 1
1) by 2.5g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml solvent a acetone, magnetic agitation 5 days at normal temperatures, rotating speed 1000rpm, obtains trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 50ml solvent b deionized water with the 1 second speed of 1 in gained solution a, caused by non-solvent and be separated, gained system is the dispersion liquid containing trifluompropyl methyl polysiloxane (PTFPMS) micro-nano aggregate, is also micro/nano level super hydrophobic coating.
Employing cotton gauze is substrate, is immersed 3-5min in micro/nano level super hydrophobic coating, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic gauze.
Fig. 1 is the scanning electron microscope (SEM) photograph of super-hydrophobic gauze prepared by this embodiment, and magnification is 330 times.
After tested, the water contact angle of super-hydrophobic gauze is greater than 150 °, to oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.) contact angle be 0 °, may be used for being separated macroscopical oil-water mixture, separation efficiency more than 98%, as shown in Figures 2 and 3.This super-hydrophobic gauze can also be used for automatically cleaning goods, water-proof material etc.
By super-hydrophobic gauze warp under atmosphere at room temperature environment 60co is that the gammairradiation 10min of the 100kGy of light source carries out cross-linking radiation, and through test after process, this gauze is still greater than 150 ° to the contact angle of water, and after soaking in the ketone such as tetrahydrofuran (THF), acetoneand ethyl acetate or esters solvent, super-hydrophobicity still can keep.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic gauze, drop is easily from its surperficial landing, after tested, this gauze to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic gauze the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this gauze to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 2
1) be that 10,000 trifluompropyl methyl polysiloxanes (PTFPMS) are dissolved in 100ml acetone by 5.0g weight-average molecular weight, under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micro-nano aggregate, is micro/nano level super hydrophobic coating.
Immersed by polypropylene non-woven fabric in this micro/nano level super hydrophobic coating and deposit 3 – 5min, dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic non-woven fabrics.After tested, the contact angle of this super-hydrophobic non-woven fabrics to water is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic non-woven fabrics can also be used as automatically cleaning goods, water-proof material etc.
Embodiment 3
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml acetone, under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Polyurethane sponge is immersed in this micro/nano level super hydrophobic coating and deposit 3 – 5min, dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely super-hydrophobic sponge is obtained, after tested, the contact angle of this super-hydrophobic sponge to water is greater than 150 °, is 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic sponge can also be used as automatically cleaning goods, water-proof material etc.
Embodiment 4
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml acetone, under the magnetic agitation of 800rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 900rpm, in step 1) dropwise add 100ml deionized water in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Entered by absorbent cotton in this micro/nano level super hydrophobic coating and deposit 3 – 5min, dry 3h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic absorbent cotton.After tested, the contact angle of this super-hydrophobic absorbent cotton to water is greater than 150 °, is 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), and may be used for the oil-water mixture being separated macroscopic view, separation efficiency is more than 98%.This super-hydrophobic sponge can also be used as automatically cleaning goods, water-proof material etc.
Embodiment 5
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml acetone, under the magnetic agitation of 900rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 700rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Loaded in watering can by this micro/nano level super hydrophobic coating, micro/nano level super hydrophobic coating is sprayed to Stainless Steel Wire net surface, and the mean pore size of described Stainless Steel Cloth is less than 200 μm, after spraying for several times, dry 2h at normal temperatures, after making solvent evaporates, namely obtains super-hydrophobic Stainless Steel Cloth.After tested, the contact angle of this super-hydrophobic Stainless Steel Cloth to water is greater than 150 °, is 0 ° to the contact angle of oil, may be used for being separated macroscopical oil-water mixture.Separation efficiency is more than 98%.This super-hydrophobic Stainless Steel Cloth can also be used as automatically cleaning goods, water-proof material etc.Due to the high-temperature stability of this super-hydrophobic coat, this super-hydrophobic Stainless Steel Cloth may be used for separating high-temp (90 – 100 DEG C) oil-water mixture.
This super-hydrophobic Stainless Steel Cloth is placed in retort furnace 400 DEG C of calcining 2h times, after tested, the contact angle of the Stainless Steel Cloth after calcining to water is greater than 150 °, has resistant to elevated temperatures characteristic.
Embodiment 6
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml acetone, under the magnetic agitation of 900rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 900rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
By centrifugal for micro/nano level super hydrophobic coating 10min, rotating speed is 12000rpm, and obtain only containing the dispersion liquid B of Micelle-like Nano-structure of Two with blue-opalescent, be also nano level super hydrophobic coating, in this nano level super hydrophobic coating, the particle diameter of aggregate is 20nm.
Nano level super hydrophobic coating is coated under 0.04MPa vacuum pressure surface and the inside of 450nm nylon membrane, after putting it into 80 DEG C of oven for drying 3h, after tested, modified nylon membrane is 120 ° at the water contact angle of air, to oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.) contact angle contact angle be 0 °, at oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.) mutually in 150 ° are greater than to the contact angle of water, it is 0 ° to the contact angle of oil, may be used for the water-in-oil emulsion being separated surfactant-free and surfactants stabilize, separation efficiency is more than 99.99%.Due to the high-temperature stability of this coating, modified nylon membrane also can be used for the water-in-oil emulsion (90 – 100 DEG C) of separating high-temp, and separation efficiency is more than 99.99%.
Embodiment 7
1) by 2.5g weight-average molecular weight be 10,000 trifluoro propyl methylsiloxane (PTFPMS) be dissolved in 100ml ethyl acetate, under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain trifluoro propyl methylsiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 50ml ethanol with the 1 second speed of 1 in gained solution a, caused by non-solvent and be separated, gained system is the dispersion liquid containing trifluoro propyl methylsiloxane (PTFPMS) micro-nano aggregate, is micro/nano level super hydrophobic coating.
Employing cotton gauze is substrate, is immersed 3 – 5min in micro/nano level super hydrophobic coating, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic gauze.After tested, the water contact angle of super-hydrophobic gauze is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic gauze can also be used for automatically cleaning goods, water-proof material etc.
Embodiment 8
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml ethyl acetate, under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 100ml ethanol with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid simultaneously containing micro-nano aggregate, is micro/nano level super hydrophobic coating.
Immersed by polypropylene non-woven fabric in this micro/nano level super hydrophobic coating and deposit 3 – 5min, the mean pore size of described non-woven fabrics is less than 200 μm, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic non-woven fabrics.After tested, the contact angle of this super-hydrophobic non-woven fabrics to water is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic non-woven fabrics can also be used as automatically cleaning goods, water-proof material etc.
By super-hydrophobic non-woven fabrics warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this non-woven fabrics is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic non-woven fabrics, drop is easily from its surperficial landing, after tested, this non-woven fabrics to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic non-woven fabrics the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this non-woven fabrics to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 9
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml ethyl acetate, under the magnetic agitation of 500rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 1000rpm, in step 1) dropwise add 100ml ethanol with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Immersed by polyurethane sponge in this micro/nano level super hydrophobic coating and deposit 3 – 5min, the mean pore size of described polyurethane sponge is less than 800 μm, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic sponge.After tested, the contact angle of this super-hydrophobic sponge to water is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic sponge can also be used as automatically cleaning goods, water-proof material etc.
By super-hydrophobic sponge warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this sponge is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic sponge, drop is easily from its surperficial landing, after tested, this sponge to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic sponge the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this sponge to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 10
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml ethyl acetate, under the magnetic agitation of 800rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 900rpm, in step 1) dropwise add 100ml ethanol with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Entered by absorbent cotton in this micro/nano level super hydrophobic coating and deposit 3 – 5min, the mean pore size of described absorbent cotton is less than 600 μm, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic absorbent cotton.After tested, the contact angle of this super-hydrophobic absorbent cotton to water is greater than 150 °, is 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), and may be used for the oil-water mixture being separated macroscopic view, separation efficiency is more than 98%.This super-hydrophobic sponge can also be used as automatically cleaning goods, water-proof material etc.
By super-hydrophobic absorbent cotton warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this absorbent cotton is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic absorbent cotton, drop is easily from its surperficial landing, after tested, this absorbent cotton to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic absorbent cotton the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this absorbent cotton to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 11
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml ethyl acetate, under the magnetic agitation of 900rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 700rpm, in step 1) dropwise add 100ml ethanol with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Load this micro/nano level super hydrophobic coating with in the bottle of nozzle, by paint spay-coating to Stainless Steel Wire net surface, the mean pore size of described Stainless Steel Cloth is less than 200 μm, after spraying for several times, dry 2h at normal temperatures, after making solvent evaporates, namely obtains super-hydrophobic Stainless Steel Cloth.After tested, the contact angle of this super-hydrophobic Stainless Steel Cloth to water is greater than 150 °, is 0 ° to the contact angle of oil, may be used for being separated macroscopical oil-water mixture.Separation efficiency is more than 98%.This super-hydrophobic Stainless Steel Cloth can also be used as automatically cleaning goods, water-proof material etc.Due to the high-temperature stability of this super-hydrophobic coat, this super-hydrophobic Stainless Steel Cloth may be used for separating high-temp (90 – 100 DEG C) oil-water mixture.
By super-hydrophobic Stainless Steel Cloth warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this Stainless Steel Cloth is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic Stainless Steel Cloth, drop is easily from its surperficial landing, after tested, this Stainless Steel Cloth to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
This super-hydrophobic Stainless Steel Wire is placed the weight that weight is 150g on the net, in 15cm distance, it is made to rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this Stainless Steel Cloth to water is greater than 150 °, has the characteristic of mechanical resistant friction.
This super-hydrophobic Stainless Steel Cloth is placed in retort furnace 400 DEG C of calcining 2h times, after tested, the contact angle of the Stainless Steel Cloth after calcining to water is greater than 150 °, has resistant to elevated temperatures characteristic.
Embodiment 12
1) by 5.0g weight-average molecular weight be 10,000 trifluompropyl methyl polysiloxane (PTFPMS) be dissolved in 100ml ethyl acetate, under the magnetic agitation of 900rpm, stir 5 days under normal temperature, obtain trifluompropyl methyl polysiloxane (PTFPMS) solution, also ie in solution a;
2) under the magnetic agitation of 900rpm, in step 1) dropwise add 100ml ethanol with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
By centrifugal for micro/nano level super hydrophobic coating 10min, rotating speed is 12000rpm, and obtain only containing the dispersion liquid B of Micelle-like Nano-structure of Two with blue-opalescent, be also nano level super hydrophobic coating, in this nano level super hydrophobic coating, the particle diameter of aggregate is 20nm.
Nano level super hydrophobic coating is coated under 0.04MPa vacuum pressure surface and the inside of 450nm nylon membrane, after putting it into 80 DEG C of oven for drying 2h, after tested, modified nylon membrane is 120 ° at the water contact angle of air, to oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.) contact angle contact angle be 0 °, at oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.) mutually in 150 ° are greater than to the contact angle of water, it is 0 ° to the contact angle of oil, may be used for the water-in-oil emulsion being separated surfactant-free and surfactants stabilize, separation efficiency is more than 99.99%.Due to the high-temperature stability of this coating, modified nylon membrane also can be used for the water-in-oil emulsion (90 – 100 DEG C) of separating high-temp, and separation efficiency is more than 99.99%.
Embodiment 13
1) by 2.5g weight-average molecular weight be 20,000 poly-methyl nine fluorine hexyl siloxanes (PNFHMS) be dissolved in 100ml tetrahydrofuran (THF), under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain poly-methyl nine fluorine hexyl siloxanes (PNFHMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 50ml deionized water with the 1 second speed of 1 in gained solution a, caused by non-solvent and be separated, gained system is the dispersion liquid containing poly-methyl nine fluorine hexyl siloxanes (PNFHMS) micro-nano aggregate, is micro/nano level super hydrophobic coating.
Employing cotton gauze is substrate, is immersed 3 – 5min in micro/nano level super hydrophobic coating, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic gauze.After tested, the water contact angle of super-hydrophobic gauze is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic gauze can also be used for automatically cleaning goods, water-proof material etc.
By super-hydrophobic gauze warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this gauze is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic gauze, drop is easily from its surperficial landing, after tested, this gauze to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic gauze the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this gauze to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 14
1) by 5.0g weight-average molecular weight be 20,000 poly-methyl nine fluorine hexyl siloxanes (PNFHMS) be dissolved in 100ml tetrahydrofuran (THF), under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain poly-methyl nine fluorine hexyl siloxanes (PNFHMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micro-nano aggregate, is micro/nano level super hydrophobic coating.
Immersed by polypropylene non-woven fabric in this micro/nano level super hydrophobic coating and deposit 3 – 5min, the mean pore size of described non-woven fabrics is less than 200 μm, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic non-woven fabrics.After tested, the contact angle of this super-hydrophobic non-woven fabrics to water is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic non-woven fabrics can also be used as automatically cleaning goods, water-proof material etc.
Embodiment 15
1) by 5.0g weight-average molecular weight be 20,000 poly-methyl nine fluorine hexyl siloxanes (PNFHMS) be dissolved in 100ml tetrahydrofuran (THF), under the magnetic agitation of 500rpm, stir 5 days under normal temperature, obtain poly-methyl nine fluorine hexyl siloxanes (PNFHMS) solution, also ie in solution a;
2) under the magnetic agitation of 1000rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Polyurethane sponge is immersed in this micro/nano level super hydrophobic coating and deposit 3 – 5min, the mean pore size of described polyurethane sponge is less than 800 μm, dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtain super-hydrophobic sponge, after tested, the contact angle of this super-hydrophobic sponge to water is greater than 150 °, to oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.) contact angle be 0 °, may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic sponge can also be used as automatically cleaning goods, water-proof material etc.
By super-hydrophobic sponge warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this sponge is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic sponge, drop is easily from its surperficial landing, after tested, this sponge to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic sponge the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this sponge to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 16
1) by 2.5g weight-average molecular weight be 20,000 poly-methyl nine fluorine hexyl siloxanes (PNFHMS) be dissolved in 100ml tetrahydrofuran (THF), under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain poly-methyl nine fluorine hexyl siloxanes (PNFHMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 50ml deionized water with the 1 second speed of 1 in gained solution a, caused by non-solvent and be separated, gained system is the dispersion liquid containing poly-methyl nine fluorine hexyl siloxanes (PNFHMS) micro-nano aggregate, is micro/nano level super hydrophobic coating.
Employing cotton gauze is substrate, is immersed 3 – 5min in micro/nano level super hydrophobic coating, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic gauze.After tested, the water contact angle of super-hydrophobic gauze is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic gauze can also be used for automatically cleaning goods, water-proof material etc.
By super-hydrophobic gauze warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this gauze is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic gauze, drop is easily from its surperficial landing, after tested, this gauze to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic gauze the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this gauze to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 17
1) by 5.0g weight-average molecular weight be 20,000 poly-methyl nine fluorine hexyl siloxanes (PNFHMS) be dissolved in 100ml tetrahydrofuran (THF), under the magnetic agitation of 1000rpm, stir 5 days under normal temperature, obtain poly-methyl nine fluorine hexyl siloxanes (PNFHMS) solution, also ie in solution a;
2) under the magnetic agitation of 500rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micro-nano aggregate, is micro/nano level super hydrophobic coating.
Immersed by polypropylene non-woven fabric in this micro/nano level super hydrophobic coating and deposit 3 – 5min, the mean pore size of described non-woven fabrics is less than 200 μm, and dry 2h at normal temperatures after taking-up, after making solvent evaporates, namely obtains super-hydrophobic non-woven fabrics.After tested, the contact angle of this super-hydrophobic non-woven fabrics to water is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic non-woven fabrics can also be used as automatically cleaning goods, water-proof material etc.
By super-hydrophobic non-woven fabrics warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this non-woven fabrics is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic non-woven fabrics, drop is easily from its surperficial landing, after tested, this non-woven fabrics to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic non-woven fabrics the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this non-woven fabrics to water is greater than 150 °, has the characteristic of mechanical resistant friction.
Embodiment 18
1) by 5.0g weight-average molecular weight be 20,000 poly-methyl nine fluorine hexyl siloxanes (PNFHMS) be dissolved in 100ml tetrahydrofuran (THF), stirring at normal temperature 5 days under the magnetic agitation of 500rpm, obtain poly-methyl nine fluorine hexyl siloxanes (PNFHMS) solution, also ie in solution a;
2) under the magnetic agitation of 1000rpm, in step 1) dropwise add 100ml deionized water with the 1 second speed of 1 in gained solution a and be separated, gained system is the dispersion liquid containing micron/nano aggregate, is micro/nano level super hydrophobic coating.
Polyurethane sponge is immersed 3 – 5min in this micro/nano level super hydrophobic coating, dry 2h at normal temperatures after taking-up, after making solvent evaporates, obtains super-hydrophobic sponge.After tested, the contact angle of this super-hydrophobic sponge to water is greater than 150 °, and be 0 ° to the contact angle of oil (kerosene, normal hexane, dimethylbenzene, n-Hexadecane etc.), may be used for being separated macroscopical oil-water mixture, separation efficiency is more than 98%.This super-hydrophobic sponge can also be used as automatically cleaning goods, water-proof material etc.
By super-hydrophobic sponge warp under atmosphere at room temperature environment 60co be the gammairradiation 10min of the 100kGy of light source carry out surface irradiation crosslinked after, it is put into successively tetrahydrofuran (THF), acetone, ethyl acetate, ethanol, normal hexane, the ultrasonic 20h of dimethylbenzene, take out post-drying, after tested, this sponge is still greater than 150 ° to the contact angle of water, possesses solvent-proof characteristic.
By the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the sodium chloride aqueous solution of pH=7 drips to the surface of this super-hydrophobic sponge, drop is easily from its surperficial landing, after tested, this sponge to the hydrochloric acid of pH=1, the sodium hydroxide of pH=14, the contact angle of the sodium-chlor drop of pH=7 is all greater than 150 °, has the characteristic of acidproof alkali salt.
Place on this super-hydrophobic sponge the weight that weight is 150g, in 15cm distance, make it rub after 40 times in sand paper (600 order) surface circulation, after tested, the contact angle of this sponge to water is greater than 150 °, has the characteristic of mechanical resistant friction.

Claims (16)

1. prepare a method for micro/nano level super hydrophobic coating, comprise the steps:
1) fluorinated silicones is dissolved in solvent a, obtain solution a;
2) to step 1) add solvent b in the mode dripped in gained solution a and be separated, gained system is described micro/nano level super hydrophobic coating;
Described solvent a is selected from least one in tetrahydrofuran (THF), acetone, ethyl acetate and butanone;
Described solvent b is selected from least one in methyl alcohol, ethanol, Virahol, water, toluene, dimethylbenzene, normal hexane and hexanaphthene.
2. method according to claim 1, it is characterized in that: described step 1) in, described fluorinated silicones is the polysiloxane that side chain contains fluorine atom, is specifically selected from trifluompropyl methyl polysiloxane, poly-methyl nine fluorine radical siloxane, at least one of gathering in ten trifluoro caprylil methicone and poly-methyl 17 fluorine decyl siloxanes;
Wherein, the weight-average molecular weight of described trifluompropyl methyl polysiloxane is 3000 – 1,000,000;
The weight-average molecular weight of described poly-methyl nine fluorine radical siloxane is 4000-200 ten thousand;
The weight-average molecular weight of described poly-ten trifluoro caprylil methicone is 5000-250 ten thousand;
The weight-average molecular weight of described poly-methyl 17 fluorine decyl siloxanes is 6000-300 ten thousand;
The mode of dissolving is stirring and dissolving; The rotating speed stirred is 100-3000rpm, is specially 800-1000rpm; The time of stirring is 1-30 days, is specially 5 days;
In described solution a, the concentration of fluorinated silicones is 0.1-200mg/ml, preferred 25-50mg/ml;
Described step 2) in, the mass ratio of described fluorinated silicones and described solvent b is 1:10-10000, preferred 1:20-600;
In described dropping step, the speed of dropping is within 1 second 1, drop to 1 second 10;
The described mode be separated is for stirring; The rotating speed stirred is 100-3000rpm, is specially 500-1000rpm.
3. the micro/nano level super hydrophobic coating for preparing of the arbitrary described method of claim 1-2.
4. micro/nano level super hydrophobic coating according to claim 3, is characterized in that: in described micro/nano level super hydrophobic coating, and the particle diameter of aggregate is 20 μ m – 20nm.
5. prepare a method for nano level super hydrophobic coating, comprise the steps: centrifugal for arbitrary for claim 3 or 4 described micro/nano level super hydrophobic coating, collect centrifugal after the supernatant liquid that obtains, obtain described nano level super hydrophobic coating.
6. method according to claim 5, is characterized in that: in described centrifugation step, and centrifugal rotational speed is 500rpm-12000rpm, centrifugation time 5min-30min, and centrifugal radius is 6-12cm.
7. the nano level super hydrophobic coating for preparing of method described in claim 5 or 6.
8. nano level super hydrophobic coating according to claim 7, is characterized in that: in described nano level super hydrophobic coating, and the particle diameter of aggregate is 20nm-100nm.
9. nano level super hydrophobic coating described in micro/nano level super hydrophobic coating described in claim 3 or 4 or claim 7 or 8 is preparing the application in superhydrophobic article;
Or, the application of nano level super hydrophobic coating described in claim 7 or 8 in the super-hydrophobic filter membrane of preparation;
Or, the superhydrophobic article prepared by nano level super hydrophobic coating described in micro/nano level super hydrophobic coating described in claim 3 or 4 or claim 7 or 8;
Or, the super-hydrophobic filter membrane prepared by nano level super hydrophobic coating described in claim 7 or 8;
Wherein, the aperture of described superhydrophobic article is 1 μm-1000 μm;
The aperture of described super-hydrophobic filter membrane is 20nm-900nm.
10. prepare a method for superhydrophobic article, comprise the steps:
Micro/nano level super hydrophobic coating described in claim 3 or 4 is flooded or is sprayed in substrate, dry, obtain described superhydrophobic article.
11. methods according to claim 10, is characterized in that: the material forming described substrate is fiber or porous material, is specially fabric, sponge, metal screen or filter paper; Wherein, described fabric is natural fabric or synthetic textile, and described natural fabric is specially cotton, fiber crops, silk or hair textiles; Described synthetic textile is terylene, polypropylene fibre, polyamide fibre, spandex or acrylic fibers textiles; Described sponge is polyester, polyvinyl alcohol foam sponge or polyethers sponge; Described metal screen to be mean pore size the be stainless (steel) wire of 30 μm-1000 μm; Described filter paper is qualitative filter paper or quantitative paper;
In described drying step, temperature is 25-100 DEG C, and the time is 1h-24h.
12. 1 kinds of methods preparing super-hydrophobic filter membrane, comprise the steps:
Nano level super hydrophobic coating described in claim 7 or 8 is coated on filter membrane under vacuum, dry, obtain described super-hydrophobic filter membrane.
13. methods according to claim 12, is characterized in that: the aperture of described filter membrane is 20nm-900nm;
Described filter membrane is nylon membrane, poly tetrafluoroethylene, polyvinylidene fluoride film, blend fiber ester film, glass fibre membrane, di-aluminium trioxide film, polyamide membrane, cellulose acetate membrane, polysulfone membrane, poly (ether sulfone) film or polyvinyl alcohol film;
In described vacuum condition, vacuum tightness is 0.02-0.1MPa;
In described drying step, temperature is 30-100 DEG C, and the time is 1h-24h.
The superhydrophobic article that 14. claims 10 or 11 prepare; Or,
The super-hydrophobic filter membrane that claim 12 or 13 prepares.
15. superhydrophobic article according to claim 14, is characterized in that: described superhydrophobic article is the superhydrophobic article with at least one in following performance: solvent resistant, acid and alkali-resistance, high temperature resistant and mechanical resistant friction;
Wherein, described high temperature resistant be the temperature of the highest tolerance 400 DEG C.
Superhydrophobic article described in 16. claims 14 or 15 or the application of super-hydrophobic filter membrane in oily water separation.
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